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栀子饮片及栀子配方颗粒的指纹图谱建立、含量测定及化学模式识别

Establishment of fingerprint,content determination and chemical pattern recognition of decoction pieces and dispensing granules of Gardenia jasminoides

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【作者】 梁朝锋韩晓珂秦亚东徐斌祁俊周娟娟

【Author】 LIANG Chaofeng;HAN Xiaoke;QIN Yadong;XU Bin;QI Jun;ZHOU Juanjuan;Drug Control Room,Wuhu Municipal Hospital of Traditional Chinese Medicine;Dept.of Pharmacy,Anhui College of Traditional Chinese Medicine;

【机构】 芜湖市中医医院药检室安徽中医药高等专科学校药学系

【摘要】 目的 建立栀子饮片及栀子配方颗粒的指纹图谱,测定其中6个成分的含量,并结合化学模式识别分析评价其质量。方法采用高效液相色谱法。以栀子苷为参照,采用《中药色谱指纹图谱相似度评价系统(2012版)》绘制20批栀子饮片及10批栀子配方颗粒的指纹图谱,并进行相似度评价,确定共有峰;同法测定去乙酰车叶草酸甲酯、栀子苷、苦番红花素、芦丁、西红花苷Ⅰ、西红花苷Ⅱ的含量;采用ORIGIN 9.1软件进行聚类分析,采用SIMCA 16.0软件进行主成分分析、偏最小二乘法-判别分析,以变量投影重要性(VIP)值大于1为标准筛选影响栀子饮片及栀子配方颗粒质量的差异性成分。结果 20批栀子饮片及10批栀子配方颗粒均有24个共有峰,30批样品共有22个共有峰,相似度均不低于0.96;共指认了6个共有峰,分别为去乙酰车叶草酸甲酯(2号峰)、栀子苷(6号峰)、苦番红花素(9号峰)、芦丁(11号峰)、西红花苷Ⅰ(15号峰)、西红花苷Ⅱ(17号峰)。栀子饮片中上述6个成分的平均含量分别为1.04、57.00、1.30、1.03、9.63、0.99 mg/g,栀子配方颗粒中的平均含量分别为0.96、17.04、0.37、0.27、0.73、0.04 mg/g。主成分分析结果显示,栀子饮片和栀子配方颗粒各分为一类,与聚类分析结果一致;有9个共有峰的VIP值>1,分别为16号峰、14号峰、3号峰、17号峰(西红花苷Ⅱ)、15号峰(西红花苷Ⅰ)、18号峰、22号峰、2号峰(去乙酰车叶草酸甲酯)、21号峰。结论 所建指纹图谱和含量测定方法简便、重复性较好,结合化学模式识别可用于评价栀子饮片及栀子配方颗粒的质量;16号峰等色谱峰对应的9个成分可能是影响两者质量的差异性成分。

【Abstract】 OBJECTIVE To establish the fingerprint of decoction pieces and dispensing granules of Gardenia jasminoides,to determine the contents of 6 components,so as to evaluate its quality combined with chemical pattern recognition. METHODS High performance liquid chromatography(HPLC) was used. Using geniposide as the reference,Similarity Evaluation System for Chromatographic Fingerprint of TCM(2012 edition)was used to draw the fingerprints of 20 batches of G. jasminoides decoction pieces and 10 batches of G. jasminoides dispensing granules. Similarity evaluation and common peaks identification were conducted. The same HPLC method was adopted to determine the contents of deacetyl asperulosidic acid methyl ester,geniposide,picrocrocin,rutin,crocin-Ⅰ and crocin-Ⅱ. ORIGIN 9.1 software was used for hierarchical clustering analysis,and SIMCA 16.0 software was used for principal component analysis(PCA) and partial least squares-discriminant analysis. The differential components affecting the quality of decoction pieces and dispensing granules were screened by taking the variable importance in projection(VIP) value>1 as the standard. RESULTS There were 24 common peaks for both 20 batches of G. jasminoides decoction piece and 10 batches of G. jasminoides dispensing granules;a total of 22 common peaks were found in the fingerprints of 30 batches of samples,and the similarity was not lower than 0.96;six common peaks were identified,i.e. deacetyl asperulosidic acid methyl ester(peak 2),geniposide(peak 6),picrocrocin(peak 9),rutin(peak 11),crocin-Ⅰ(peak 15),crocin-Ⅱ(peak17). Average contents of above 6 components in G. jasminoides decoction pieces were 1.04,57.00,1.30,1.03,9.63 and 0.99 mg/g,respectively;those of G. jasminoides dispensing granules were 0.96,17.04,0.37,0.27,0.73 and 0.04 mg/g,respectively. PCA results showed that G. jasminoides decoction pieces and G.jasminoides dispensing granules were clustered into respective one category, which was consistent with results of cluster analysis. There were 9 common peaks with VIP value>1,which were 16,14,3,17(crocin-Ⅱ),15(crocin-Ⅰ),18,22, 2(deacetyl asperulosidic acid methyl ester) and 21.CONCLUSIONS The established fingerprint and content determination method are simple and reproducible. Combined with chemical pattern recognition,it can be used to evaluate the quality of decoction pieces and dispensing granules of G. jasminoides.Nine corresponding components represented by peak 16 and so on are the differential components that affect the quality of them.

【基金】 中央补助安徽省中医药公共卫生专项-中药炮制技术传承基地建设项目(No.卫办秘[2016]531号);安徽省教育厅高校学科(专业)拔尖人才学术资助项目(No.gxbj ZD2021103);芜湖市华佗计划卫生高层次人才分层培养项目(No.芜卫组[2021]134号)
  • 【分类号】R286.0
  • 【下载频次】411
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